Tetra­kis[(4-meth­oxy­carbon­yl)anilinium] hexa­chloridostannate(IV) dichloride

Wenzhi Xiao; Ruiting Xue; Yansheng Yin

doi:10.1107/S1600536811003692

. 2011 Feb 2;67(Pt 3):m297. doi: 10.1107/S1600536811003692

Tetrakis[(4-methoxycarbonyl)anilinium] hexachloridostannate(IV) dichloride

Wenzhi Xiao ^a, Ruiting Xue ^b, Yansheng Yin ^b,^*

PMCID: PMC3052157 PMID: 21522237

Abstract

The asymmetric unit of the title compound, (C₈H₁₀NO₂)₄[SnCl₆]Cl₂, contains two (4-methoxycarbonyl)anilinium cations, one chloride anion and one half of a hexachloridostannate(IV) dianion situated on a twofold rotation axis. All aminium H atoms are involved in N—H⋯Cl hydrogen bonding, which consolidate the crystal packing along with weak C—H⋯O interactions.

Related literature

For general background to inorganic–organic hybrid compounds, see: Zhang et al. (2009 ▶); Descalzo et al. (2006 ▶); Li et al. (2007 ▶), Sanchez et al. (2005 ▶).

Experimental

Crystal data

(C₈H₁₀NO₂)₄[SnCl₆]Cl₂
M _r = 1010.97
Monoclinic,
a = 30.748 (3) Å
b = 7.1172 (8) Å
c = 22.113 (2) Å
β = 119.424 (2)°
V = 4215.0 (7) Å³
Z = 4
Mo Kα radiation
μ = 1.16 mm⁻¹
T = 298 K
0.50 × 0.46 × 0.46 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.594, T _max = 0.617
10221 measured reflections
3719 independent reflections
2969 reflections with I > 2σ(I)
R _int = 0.035

Refinement

R[F ² > 2σ(F ²)] = 0.031
wR(F ²) = 0.090
S = 1.01
3719 reflections
245 parameters
H-atom parameters constrained
Δρ_max = 0.51 e Å⁻³
Δρ_min = −0.44 e Å⁻³

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811003692/cv5035sup1.cif

e-67-0m297-sup1.cif^{(18.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811003692/cv5035Isup2.hkl

e-67-0m297-Isup2.hkl^{(182.4KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯Cl3	0.89	2.78	3.659 (4)	170
N2—H2B⋯Cl3	0.89	2.71	3.479 (3)	145
N2—H2C⋯Cl4	0.89	2.21	3.098 (4)	177
N1—H1B⋯Cl4ⁱ	0.89	2.29	3.155 (4)	165
N1—H1C⋯Cl4ⁱⁱ	0.89	2.22	3.092 (4)	166
N2—H2A⋯Cl1ⁱⁱⁱ	0.89	3.01	3.482 (3)	115
C3—H3⋯O4^iv	0.93	2.39	3.148 (6)	139
C15—H15⋯O2^v	0.93	2.38	3.130 (5)	138

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) .

Acknowledgments

The authors acknowledge the financial support of the National Science Foundation of China (grant Nos. 50672090 and 50702053).

supplementary crystallographic information

Comment

Considerable attention has been devoted to inorganic-organic hybrid materials over recent years (Zhang et al., 2009). These hybrid materials have potential applications in many areas including gas storage, separation, catalysis, magnetism, optics as well as electrical conductivity (Descalzo et al., 2006; Li et al., 2007; Sanchez et al., 2005]. Herein we report the structure of the title compound (Fig.1.),

This title compound contains SnCl₆ inorganic anions, organic cations and dissociated chloride anions. The SnCl₆ inorganic anion adopts a regular octahedron geometry, with average Sn—Cl distance of 2.4262 Å. In the organic cation, the dihedral angle between the ester group and the phenyl ring is 14.86(0.19)°.

In the crystal structure, intermolecular N—H···Cl and C—H···O hydrogen bonds (Table 1) link cations and anions into layers with alternating inorganic and organic species.

Experimental

4-Aminobenzoic acid (10 mmol) was dissolved to acid methanol solution (10 ml). Ten minutes later, a methanol solution (10 ml) of tin tetrachloride(5 mmol) was added with stirring. The mixture was stirred for 4 h. Crystals of the title compound suitable for X-ray analysis were grown from the saturation ethanol solution after about two weeks.